Baw sensor device with peel-resistant wall structure

ABSTRACT

Lateral boundaries of a fluidic passage of a fluidic device incorporating at least one BAW resonator structure are fabricated with photosensitive materials (e.g., photo definable epoxy, solder mask resist, or other photoresist), allowing for high aspect ratio, precisely dimensioned walls. Resistance to delamination and peeling between a wall structure and a base structure is enhanced by providing a wall structure that includes a thin footer portion having a width that exceeds a width of an upper wall portion extending upward from the footer portion, and/or by providing a wall structure arranged over at least one anchoring region of a base structure. Anchoring features may include recesses and/or protrusions.

STATEMENT OF RELATED APPLICATIONS

This application claims the benefit of provisional patent applicationSer. No. 62/266,973, filed Dec. 14, 2015, the disclosure of which ishereby incorporated herein by reference in its entirety.

TECHNICAL FIELD

The present disclosure relates to fluidic devices incorporating acousticresonators, including fluidic devices and related systems suitable forbiosensing or biochemical sensing applications.

BACKGROUND

A biosensor (or biological sensor) is an analytical device including abiological element and a transducer that converts a biological responseinto an electrical signal. Certain biosensors involve a selectivebiochemical reaction between a specific binding material (e.g., anantibody, a receptor, a ligand, etc.) and a target species (e.g.,molecule, protein, DNA, virus, bacteria, etc.), and the product of thishighly specific reaction is converted into a measurable quantity by atransducer. Other sensors may utilize a non-specific binding materialcapable of binding multiple types or classes of molecules or othermoieties that may be present in a sample, such as may be useful inchemical sensing applications. The term “functionalization material” maybe used herein to generally relate to both specific and non-specificbinding materials. Transduction methods may be based on variousprinciples, such as electrochemical, optical, electrical, acoustic, andso on. Among these, acoustic transduction offers a number of potentialadvantages, such as being real time, label-free, and low cost, as wellas exhibiting high sensitivity.

An acoustic wave device employs an acoustic wave that propagates throughor on the surface of a piezoelectric material, whereby any changes tothe characteristics of the propagation path affect the velocity and/oramplitude of the wave. Presence of functionalization material embodiedin a specific binding material along an active region of an acousticwave device permits a specific analyte to be bound to the specificbinding material, thereby altering the mass being vibrated by theacoustic wave and altering the wave propagation characteristics (e.g.,velocity, thereby altering resonance frequency). Changes in velocity canbe monitored by measuring the frequency, amplitude-magnitude, or phasecharacteristics of the acoustic wave device, and can be correlated to aphysical quantity being measured.

In the case of a piezoelectric crystal resonator, an acoustic wave mayembody either a bulk acoustic wave (BAW) propagating through theinterior of a piezoelectric material, or a surface acoustic wave (SAW)propagating on the surface of the piezoelectric material. SAW devicesinvolve transduction of acoustic waves (commonly includingtwo-dimensional Rayleigh waves) utilizing interdigital transducers alongthe surface of a piezoelectric material, with the waves being confinedto a penetration depth of about one wavelength. BAW devices typicallyinvolve transduction of an acoustic wave using electrodes arranged onopposing top and bottom surfaces of a piezoelectric material. In a BAWdevice, three wave modes can propagate, namely, one longitudinal mode(embodying longitudinal waves, also called compressional/extensionalwaves), and two shear modes (embodying shear waves, also calledtransverse waves), with longitudinal and shear modes respectivelyidentifying vibrations where particle motion is parallel to orperpendicular to the direction of wave propagation. The longitudinalmode is characterized by compression and elongation in the direction ofthe propagation, whereas the shear modes consist of motion perpendicularto the direction of propagation with no local change of volume.Longitudinal and shear modes propagate at different velocities. Inpractice, these modes are not necessarily pure modes, as the particlevibration, or polarization, is neither purely parallel nor purelyperpendicular to the propagation direction. The propagationcharacteristics of the respective modes depend on the materialproperties and propagation direction respective to the c-axisorientations. The ability to create shear displacements is beneficialfor operation of acoustic wave devices with fluids (e.g., liquids)because shear waves do not impart significant energy into fluids.

Certain piezoelectric thin films are capable of exciting bothlongitudinal and shear mode resonance, such as hexagonal crystalstructure piezoelectric materials including (but not limited to)aluminum nitride (AlN) and zinc oxide (ZnO). To excite a wave includinga shear mode using a piezoelectric material arranged between electrodes,a polarization axis in a piezoelectric thin film must generally benon-perpendicular to (e.g., tilted relative to) the film plane. Inbiological sensing applications involving liquid media, the shearcomponent of the resonator is used. In such applications, piezoelectricmaterial may be grown with a c-axis orientation distribution that isnon-perpendicular relative to a face of an underlying substrate toenable a BAW resonator structure to exhibit a dominant shear responseupon application of an alternating current signal across electrodesthereof.

Typically, BAW devices are fabricated by micro-electro-mechanicalsystems (MEMS) fabrication techniques owing to the need to providemicroscale features suitable for facilitating high frequency operation.In the context of biosensors, functionalization materials (e.g.,specific binding materials; also known as bioactive probes or agents)may be deposited on sensor surfaces by microarray spotting (also knownas microarray printing) using a microarray spotting needle.Functionalization materials providing non-specific binding utility(e.g., permitting binding of multiple types or species of molecules) mayalso be used in certain contexts, such as chemical sensing.

Sensing devices incorporating BAW resonator structures and intended foruse with fluids may define fluidic passages to direct fluid over anactive region. Structures defining fluidic passages may incorporate wallstructures and cover structures. The small dimensions associated withsensing regions may render it challenging to fabricate wall structuresthat (i) define fluidic passages appropriately aligned with resonatoractive regions without occlusion and (ii) resist peeling from anunderlying substrate. For example, when inter-layer adhesives are usedto assemble precut layers (e.g., including wall layers) of a multi-layersensing device, it may be difficult to provide adhesive in a sufficientamount to promote proper adhesion without providing excess adhesive thatmay flow into a fluidic passage. Alternatively, if curable materials areused to define wall structures of a sensing device, it may bechallenging to promote persistent bonding between the wall structuresand a substrate (and thereby preventing peeling of the wall structures),particularly when wall structures having elevated wall height/widthaspect ratios are provided, and when wall structures are exposed tofluids and/or humid operating environments.

Accordingly, there is a need for devices incorporating bulk acousticwave resonator structures suitable for operation in the presence ofliquid for biosensing or biochemical sensing applications that overcomelimitations associated with conventional devices.

SUMMARY

The present disclosure provides fluidic devices incorporating BAWresonator structures with wall structures that resist peeling (e.g.,delamination) from a base structure. One or more wall structures definelateral boundaries of a fluidic passage arranged to receive a fluid andcontaining an active region of a BAW resonator structure, wherein thewall structures may be advantageously produced with photoresist (e.g.,SU-8) or epoxy materials. In certain embodiments, peel resistance isenhanced by providing a wall structure that includes a footer portionhaving a width that exceeds a width of an upper wall portion extendingupward from the footer portion. In certain embodiments, peel resistanceis enhanced by providing a wall structure arranged over at least oneanchoring region of a base structure, wherein the at least one anchoringregion includes at least one anchoring feature, and the at least oneanchoring feature includes at least one recess and/or at least oneprotrusion (optionally, multiple recesses and/or multiple protrusions).In certain embodiments, peel resistance may be further enhanced byproviding a wall structure including a footer portion having a widththat exceeds a width of an upper wall portion, with the footer portionbeing arranged over at least one anchoring region of a base structure.Methods for fabricating a fluidic device as disclosed herein, as well asmethods for biological or chemical sensing using such a fluidic device,are further provided.

In one aspect, the disclosure relates to a fluidic device comprising abase structure and a wall structure that includes a footer portion andan upper wall portion. In particular, the base structure comprises: (i)a substrate; and (ii) at least one bulk acoustic wave resonatorstructure supported by the substrate, the at least one bulk acousticwave resonator structure including a piezoelectric material, a top sideelectrode arranged over a portion of the piezoelectric material, and abottom side electrode arranged below at least a portion of thepiezoelectric material, wherein a portion of the piezoelectric materialis arranged between the top side electrode and the bottom side electrodeto form an active region. The wall structure is arranged over at least aportion of the base structure and defines lateral boundaries of afluidic passage arranged to receive a fluid and containing the activeregion, wherein: the wall structure comprises a footer portion and anupper wall portion that protrudes upward from the footer portion; thefooter portion is arranged between the upper wall portion and the basestructure; and the footer portion comprises a width that exceeds a widthof the upper wall portion.

In certain embodiments, the fluidic device further includes a coverstructure arranged over the wall structure and defining an upperboundary of the fluidic passage.

In certain embodiments, the wall structure and the cover structure areembodied in a monolithic body structure. In certain embodiments, thewall structure comprises at least one of a photosensitive material,photoresist, or epoxy.

In certain embodiments, the fluidic device further includes at least onefunctionalization material arranged over at least a portion of theactive region. In certain embodiments, the fluidic device furtherincludes a self-assembled monolayer arranged between the at least onefunctionalization material and the top side electrode. In certainembodiments, the fluidic device further includes an interface layerarranged between the self-assembled monolayer and the top sideelectrode. In certain embodiments, the fluidic device further includes ahermeticity layer arranged between the interface layer and the top sideelectrode.

In certain embodiments, the piezoelectric material comprises a c-axishaving an orientation distribution that is predominantly non-parallel tonormal of a face of the substrate.

In another aspect, the disclosure relates to a fluidic device comprisinga base structure including at least one anchoring feature (e.g., atleast one recess and/or at least one protrusion), and a wall structurearranged over the at least one anchoring region and defining lateralboundaries of a fluidic passage arranged to receive a fluid. Inparticular, the base structure comprises: (i) a substrate; and (ii) atleast one bulk acoustic wave resonator structure supported by thesubstrate, the at least one bulk acoustic wave resonator structureincluding a piezoelectric material, a top side electrode arranged over aportion of the piezoelectric material, and a bottom side electrodearranged below at least a portion of the piezoelectric material, whereina portion of the piezoelectric material is arranged between the top sideelectrode and the bottom side electrode to form an active region, andwherein a portion of the base structure comprises at least one anchoringregion including at least one anchoring feature, and the at least oneanchoring feature comprises at least one of: (i) at least one recess or(ii) at least one protrusion. The wall structure is arranged over the atleast one anchoring region and defines lateral boundaries of a fluidicpassage arranged to receive a fluid and containing the active region.

In certain embodiments, the at least one anchoring feature comprises avertical dimension of least about 1 micron. In certain embodiments, theat least one recess comprises a plurality of recesses, and the at leastone protrusion comprises a plurality of protrusions

In certain embodiments, the fluidic device further comprises a coverstructure arranged over the wall structure and defining an upperboundary of the fluidic passage. In certain embodiments, the wallstructure and the cover structure are embodied in a monolithic bodystructure. In certain embodiments, the wall structure comprises at leastone of a photosensitive material, photoresist, or epoxy

In certain embodiments, the fluidic device further includes at least onefunctionalization material arranged over at least a portion of theactive region. In certain embodiments, the fluidic device furtherincludes a self-assembled monolayer arranged between the at least onefunctionalization material and the top side electrode. In certainembodiments, the fluidic device further includes an interface layerarranged between the self-assembled monolayer and the top sideelectrode. In certain embodiments, the fluidic device further includes ahermeticity layer arranged between the interface layer and the top sideelectrode.

In another aspect, a method for biological or chemical sensingcomprises: supplying a fluid containing an analyte into the fluidicpassage of a fluidic device disclosed herein, wherein said supplying isconfigured to cause at least some of the analyte to bind to the at leastone functionalization material; inducing a bulk acoustic wave in theactive region; and sensing a change in at least one of anamplitude-magnitude property, a frequency property, or a phase propertyof the at least one bulk acoustic wave resonator structure to indicateat least one of presence or quantity of target species bound to the atleast one functionalization material.

In another aspect, any one or more aspects or features of one or moreembodiments may be combined with aspects or features of one or moreother embodiments for additional advantage, unless indicated to thecontrary herein

Those skilled in the art will appreciate the scope of the presentdisclosure and realize additional aspects thereof after reading thefollowing detailed description of the preferred embodiments inassociation with the accompanying drawing figures.

BRIEF DESCRIPTION OF THE DRAWINGS

The accompanying drawing figures incorporated in and forming a part ofthis specification illustrate several aspects of the disclosure, andtogether with the description serve to explain the principles of thedisclosure.

FIG. 1 is a schematic cross-sectional view of a portion of a bulkacoustic wave (BAW) MEMS resonator device usable for fabricating fluidicdevices according to embodiments disclosed herein, including an activeregion with a piezoelectric material arranged between overlappingportions of a top side electrode and a bottom side electrode.

FIG. 2 is a schematic cross-sectional view of an upper portion of a BAWMEMS resonator device including a piezoelectric material and a top sideelectrode overlaid with a hermeticity layer, an interface layer, aself-assembled monolayer, and a functionalization (e.g., specificbinding) material.

FIG. 3 is a side cross-sectional schematic view of a portion of afluidic device (e.g., a biochemical sensor device) fabricated withlaser-cut laminate layers including a fluidic passage bounded from belowby a base structure including a BAW resonator structure, boundedlaterally by a wall layer, and bounded from above by a cover or caplayer, showing incursion of excess inter-layer adhesive into the fluidicpassage and serving as a first comparison device intended to providecontext for subsequently described embodiments of the disclosure.

FIG. 4A is a schematic cross-sectional view of a portion of a fluidicdevice (e.g., a biochemical sensor device) including a fluidic passagebounded from below by a base structure including a BAW resonatorstructure, bounded laterally by a wall structure fabricated ofphotosensitive (e.g., epoxy or photoresist) materials, and bounded fromabove by a cover or cap layer, serving as a second comparison deviceintended to provide context for subsequently described embodiments ofthe disclosure.

FIG. 4B is a schematic cross-sectional view of the fluidic deviceportion of FIG. 4A, showing a delamination crack between a left sidewall structure and the base structure.

FIG. 5 is a scanning electron microscope (10,000 times magnification) ofa base portion of an epoxy- or resist-based wall structure proximate toa base structure, showing a delamination crack between the wallstructure and the base structure after exposure to a humidity source.

FIG. 6A is a schematic cross-sectional view of a portion of a fluidicdevice (e.g., a biochemical sensor device) including a fluidic passagebounded from below by a base structure including a BAW resonatorstructure, bounded from above by a cover or cap layer, and boundedlaterally by a wall structure fabricated with photo-defined epoxy orresist materials, with the wall structure including a footer portionhaving a width that exceeds a width of an upper wall portion, accordingto one embodiment.

FIG. 6B is a magnified cross-sectional schematic view of an upperportion of the portion of the fluidic device shown in FIG. 6A.

FIG. 7 is a schematic cross-sectional view of a portion of a fluidicdevice (e.g., a biochemical sensor device) including a fluidic passagebounded from below by a base structure including a BAW resonatorstructure, bounded from above by a cover or cap layer, and boundedlaterally by a wall structure fabricated from photo-defined epoxy orresist materials, with the wall structure overlying anchoring regionsincluding recesses and/or protrusions defined in or on the basestructure, according to one embodiment.

FIG. 8A is a magnified schematic cross-sectional view of a singleprotrusion (i.e., an anchoring feature) formed by an interface layer andan overlying self-assembled monolayer of a fluidic device, according toone embodiment.

FIG. 8B is a magnified schematic cross-sectional view of a singleprotrusion (i.e., an anchoring feature) formed by a deposited material(e.g., photosensitive or photoimageable material) extending upward froma surface of an interface layer and being overlaid with a self-assembledmonolayer, according to one embodiment.

FIGS. 9A-9E provide schematic cross-sectional views of anchoringfeatures producible by a subtractive process in various states offormation according to one embodiment.

FIG. 10 is a schematic cross-sectional view of a portion of a fluidicdevice (e.g., a biochemical sensor device) including a fluidic passagebounded from below by a base structure including a BAW resonatorstructure, bounded from above by a cover or cap layer, and boundedlaterally by a wall structure fabricated with photo-defined epoxy orresist materials, with the wall structure including a footer portionhaving a width that exceeds a width of an upper wall portion, and withthe footer portion overlying anchoring regions including recesses and/orprotrusions defined in or on the base structure, according to oneembodiment.

FIG. 11A is a schematic cross-sectional view of a film bulk acousticwave resonator (FBAR) structure usable in devices according to certainembodiments, with the FBAR structure including an inclined c-axishexagonal crystal structure piezoelectric material, a substrate defininga cavity optionally covered by a support layer, and an active regionregistered with the cavity, with a portion of the piezoelectric materialarranged between overlapping portions of a top side electrode and abottom side electrode.

FIG. 11B is a schematic cross-sectional view of the FBAR structureaccording to FIG. 11A, following addition of a hermeticity layer, aninterface layer, a self-assembled monolayer, and a functionalization(e.g., specific binding) material over at least portions of the FBARstructure.

FIG. 12 is a top plan view photograph of a bulk acoustic wave MEMSresonator device suitable for receiving a hermeticity layer, aninterface layer, a self-assembled monolayer, and functionalization (e.g.specific binding) material as disclosed herein.

FIG. 13 is a perspective view of a base structure including multiplebulk acoustic wave MEMS resonator structures as disclosed herein,suitable for receiving a wall structure and a cover structure asdisclosed herein in order to fabricate a multi-resonator fluidic device.

DETAILED DESCRIPTION

The embodiments set forth below represent the necessary information toenable those skilled in the art to practice the embodiments andillustrate the best mode of practicing the embodiments. Upon reading thefollowing description in light of the accompanying drawing figures,those skilled in the art will understand the concepts of the disclosureand will recognize applications of these concepts not particularlyaddressed herein. It should be understood that these concepts andapplications fall within the scope of the disclosure and theaccompanying claims.

It should be understood that, although the terms first, second, etc. maybe used herein to describe various elements, these elements should notbe limited by these terms. These terms are only used to distinguish oneelement from another. For example, a first element could be termed asecond element, and, similarly, a second element could be termed a firstelement, without departing from the scope of the present disclosure. Asused herein, the term “and/or” includes any and all combinations of oneor more of the associated listed items.

It should also be understood that when an element is referred to asbeing “connected” or “coupled” to another element, it can be directlyconnected or coupled to the other element or intervening elements may bepresent. In contrast, when an element is referred to as being “directlyconnected” or “directly coupled” to another element, there are nointervening elements present.

It should be understood that, although the terms “upper,” “lower,”“bottom,” “intermediate,” “middle,” “top,” and the like may be usedherein to describe various elements, these elements should not belimited by these terms. These terms are only used to distinguish oneelement from another. For example, a first element could be termed an“upper” element and, similarly, a second element could be termed an“upper” element depending on the relative orientations of theseelements, without departing from the scope of the present disclosure.

The terminology used herein is for the purpose of describing particularembodiments only and is not intended to be limiting of the disclosure.As used herein, the singular forms “a,” “an,” and “the” are intended toinclude the plural forms as well, unless the context clearly indicatesotherwise. It will be further understood that the terms “comprises,”“comprising,” “includes,” and/or “including” when used herein specifythe presence of stated features, integers, steps, operations, elements,and/or components, but do not preclude the presence or addition of oneor more other features, integers, steps, operations, elements,components, and/or groups thereof.

Unless otherwise defined, all terms (including technical and scientificterms) used herein have the same meaning as commonly understood by oneof ordinary skill in the art to which this disclosure belongs. It willbe further understood that terms used herein should be interpreted ashaving meanings that are consistent with their meanings in the contextof this specification and the relevant art and will not be interpretedin an idealized or overly formal sense unless expressly so definedherein.

The present disclosure provides fluidic devices incorporating BAWresonator structures with wall structures that resist peeling (e.g.,delamination) from a base structure. One or more wall structures definelateral boundaries of a fluidic passage arranged to receive a fluid andcontaining an active region of a BAW resonator structure, wherein thewall structures may be advantageously produced with photoresist (e.g.,SU-8) or epoxy materials. In certain embodiments, peel resistance isenhanced by providing a wall structure that includes a footer portionhaving a width that exceeds a width of an upper wall portion extendingupward from the footer portion. In certain embodiments, peel resistanceis enhanced by providing a wall structure arranged over at least oneanchoring region of a base structure, wherein the at least one anchoringregion includes at least one anchoring feature, and the at least oneanchoring feature includes at least one recess and/or at least oneprotrusion (optionally, multiple recesses and/or multiple protrusions).In certain embodiments, peel resistance may be further enhanced byproviding a wall structure including a footer portion having a widththat exceeds a width of an upper wall portion, with the footer portionbeing arranged over at least one anchoring region of a base structure.Methods for fabricating a fluidic device as disclosed herein, as well asmethods for biological or chemical sensing using such a fluidic device,are further provided.

In certain embodiments, a BAW resonator structure comprises a hexagonalcrystal structure piezoelectric material (e.g., aluminum nitride or zincoxide) that includes a c-axis having an orientation distribution that isnon-parallel (and also non-perpendicular) to normal of a face of asubstrate over which the piezoelectric material is formed, therebyproviding a quasi-shear mode acoustic resonator. Under appropriateconditions, presence of a c-axis having an orientation distribution thatis predominantly non-parallel to normal of a face of a substrate enablesa BAW resonator structure to be configured to exhibit a dominant shearresponse upon application of an alternating current signal across a topside electrode and a bottom side electrode. Methods for forminghexagonal crystal structure piezoelectric materials including a c-axishaving an orientation distribution that is predominantly non-parallel tonormal of a face of a substrate are disclosed in U.S. patent applicationSer. No. 15/293,063 filed on Oct. 13, 2016, with the foregoingapplication hereby being incorporated by reference herein. Additionalmethods for forming piezoelectric material having an inclined c-axisorientation are disclosed in U.S. Pat. No. 4,640,756 issued on Feb. 3,1987, with the foregoing patent hereby being incorporated by referenceherein.

Before describing fluidic devices incorporating BAW resonator structuresand including wall structures that resist peeling (e.g., delamination)from a base structure, exemplary bulk acoustic wave MEMS resonatordevices, associated layers useful for providing biochemical sensingutility, and fluidic devices incorporating MEMS resonator devices willbe introduced.

Micro-electrical-mechanical system (MEMS) resonator devices according tocertain embodiments include a substrate, a BAW resonator structurearranged over at least a portion of the substrate, and afunctionalization material arranged over at least a portion of an activeregion of the BAW resonator structure. Various layers may be arrangedbetween the functionalization material and a top side electrode (whichis coincident with the active region of the BAW resonator structure),such as: a hermeticity layer (e.g., to protect the top side electrodefrom corrosion in a liquid environment), an interface layer, and/or aself-assembled monolayer (SAM), with the interface layer and/or the SAMbeing useful to facilitate attachment of at least one overlying materiallayer, ultimately including functionalization material. In certainembodiments, the interface layer facilitates attachment of an overlyingSAM, and the SAM facilitates attachment of an overlyingfunctionalization material. In certain embodiments, multiplefunctionalization materials may be provided.

FIG. 1 is a schematic cross-sectional view of a portion of a bulkacoustic wave (BAW) MEMS resonator device 10 useable for fabricatingfluidic devices according to at least certain embodiments disclosedherein. The resonator device 10 includes a substrate 12 (e.g., typicallysilicon or another semiconductor material), an acoustic reflector 14arranged over the substrate 12, a piezoelectric material 22, and bottomand top side electrodes 20, 28. The bottom side electrode 20 is arrangedalong a portion of a lower surface 24 of the piezoelectric material 22(between the acoustic reflector 14 and the piezoelectric material 22),and the top side electrode 28 is arranged along a portion of an uppersurface 26 of the piezoelectric material 22. An area in which thepiezoelectric material 22 is arranged between overlapping portions ofthe top side electrode 28 and the bottom side electrode 20 is consideredan active region 30 of the resonator device 10. The acoustic reflector14 serves to reflect acoustic waves and therefore reduce or avoid theirdissipation in the substrate 12. In certain embodiments, the acousticreflector 14 includes alternating thin layers 16, 18 of materials (e.g.,silicon oxicarbide [SiOC], silicon nitride [Si₃N₄], silicon dioxide[SiO₂], aluminum nitride [AlN], tungsten [W], and molybdenum [Mo])having different acoustic impedance values, optionally embodied in aquarter-wave Bragg mirror, deposited over the substrate 12. In certainembodiments, other types of acoustic reflectors may be used. Steps forforming the resonator device 10 may include depositing the acousticreflector 14 over the substrate 12, followed by deposition of the bottomside electrode 20, followed by growth (e.g., via sputtering or otherappropriate methods) of the piezoelectric material 22, followed bydeposition of the top side electrode 28. In certain embodiments, thepiezoelectric material 22 comprises a hexagonal crystal structurepiezoelectric material (e.g., aluminum nitride or zinc oxide) thatincludes a c-axis having an orientation distribution that ispredominantly non-parallel to (and may also be non-perpendicular to)normal of a face of the substrate 12.

The bulk acoustic wave MEMS resonator device 10 shown in FIG. 1 lacksany layers (e.g., including functionalization material) overlying theactive region 30 that would permit the resonator device 10 to be used asa biochemical sensor. If desired, at least portions of the resonatordevice 10 shown in FIG. 1 (e.g., including the active region 30) may beoverlaid with various layers, such as one or more of: a hermeticitylayer, an interface layer, a self-assembled monolayer (SAM), and/or afunctionalization material (which may include specific binding materialor non-specific binding material).

FIG. 2 is a schematic cross-sectional view of an upper portion of a BAWMEMS resonator device including a piezoelectric material 22 and a topside electrode 28 overlaid with a hermeticity layer 32, an interfacelayer 34, a self-assembled monolayer (SAM) 36, and a functionalization(e.g., specific binding) material 38. In certain embodiments, one ormore blocking materials (not shown) may be applied during fabrication,such as over portions of the interface layer 34 to prevent localizedattachment of one or more subsequently deposited layers, or (if appliedover selected regions of the SAM 36 or functionalization material 38) toprevent analyte capture in regions not overlying the active region 30 ofthe BAW MEMS resonator device.

In certain embodiments, photolithography may be used to promotepatterning of interface material or blocking material over portions of aMEMS resonator device. Photolithography involves use of light totransfer a geometric pattern from a photomask to a light-sensitivechemical photoresist on a substrate and is a process well known to thoseof ordinary skill in the semiconductor fabrication art. Typical stepsemployed in photolithography include wafer cleaning, photoresistapplication (involving either positive or negative photoresist), maskalignment, and exposure and development. After features are defined inphotoresist on a desired surface, an interface layer may be patterned byetching in one or more gaps in a photoresist layer, and the photoresistlayer may be subsequently removed (e.g., by using a liquid photoresiststripper, by ashing via application of an oxygen-containing plasma, oranother removal process).

In certain embodiments, an interface layer (e.g., arrangeable between atop side electrode and a SAM) includes a hydroxylated oxide surfacesuitable for formation of an organosilane SAM. A preferred interfacelayer material including a hydroxylated oxide surface is silicon dioxide[SiO₂]. Alternative materials incorporating hydroxylated oxide surfacesfor forming interface layers include titanium dioxide [TiO₂], tantalumpentoxide [Ta₂O₅], hafnium oxide [HfO₂], or aluminum oxide [Al₂O₃].Other alternative materials incorporating hydroxylated oxide surfaceswill be known to those skilled in the art, and these alternatives areconsidered to be within the scope of the present disclosure.

In other embodiments, an interface layer (e.g., arrangeable between atop side electrode and a SAM), or at least one electrode that is devoidof an overlying interface layer, includes gold or another noble metal(e.g., ruthenium, rhodium, palladium, osmium, iridium, platinum, orsilver) suitable for receiving a thiol-based SAM that may be overlaidwith functionalization material.

In certain embodiments incorporating electrode materials subject tocorrosion, a hermeticity layer may be applied between a top sideelectrode and an interface layer. A hermeticity layer may be unnecessarywhen noble metals (e.g., gold, platinum, etc.) are used for top sideelectrodes. If provided, a hermeticity layer preferably includes adielectric material with a low water vapor transmission rate (e.g., nogreater than 0.1 g/m²/day). Following deposition of a hermeticity layerand an interface layer, a SAM may be formed over the interface layer,with the SAM including an organosilane material in certain embodiments.The hermeticity layer protects a reactive electrode material (e.g.,aluminum or aluminum alloy) from attack in corrosive liquidenvironments, and the interface layer facilitates proper chemicalbinding of the SAM.

In certain embodiments, a hermeticity layer and/or an interface layermay be applied via one or more deposition processes such as atomic layerdeposition (ALD), chemical vapor deposition (CVD), or physical vapordeposition (PVD). Of the foregoing processes, ALD is preferred fordeposition of at least the hermeticity layer (and may also be preferablefor deposition of the interface layer) due to its ability to provideexcellent conformal coating with good step coverage over device featuresso as to provide layer structures that are free of pinholes. Moreover,ALD is capable of forming uniformly thin layers that provide relativelylittle damping of acoustic vibrations that would otherwise result indegraded device performance. Adequacy of coverage is important for ahermeticity layer (if present) to avoid corrosion of the underlyingelectrode. If ALD is used for deposition of a hermeticity layer, then incertain embodiments a hermeticity layer may include a thickness in arange of from about 10 nm to about 25 nm. In certain embodiments,hermeticity layer thickness is about 15 nm, or from about 12 nm to about18 nm. Conversely, if another process such as chemical vapor depositionis used, then a hermeticity layer may include a thickness in a range offrom about 80 nm to about 150 nm or more, or in a range of from about 80nm to about 120 nm. Considering both of the foregoing processes,hermeticity layer thicknesses may range from about 5 nm to about 150 nm.If ALD is used for deposition of an interface layer, then an interfacelayer may include a thickness in a range of from about 5 nm to about 15nm. In certain embodiments, an interface layer may include a thicknessof about 10 nm, or in a range of from about 8 nm to about 12 nm. Otherinterface layer thickness ranges and/or deposition techniques other thanALD may be used in certain embodiments. In certain embodiments, ahermeticity layer and an interface layer may be sequentially applied ina vacuum environment, thereby promoting a high-quality interface betweenthe two layers.

If provided, a hermeticity layer may include an oxide, a nitride, or anoxynitride material serving as a dielectric material and having a lowwater vapor transmission rate (e.g., no greater than 0.1 g/m²/day)according to certain embodiments. In certain embodiments, a hermeticitylayer includes at least one of aluminum oxide [Al₂O₃] or silicon nitride[SiN]. In certain embodiments, an interface layer includes at least oneof SiO₂, TiO₂, or Ta₂O₅. In certain embodiments, multiple materials maybe combined in a single hermeticity layer, and/or a hermeticity layermay include multiple sublayers of different materials. Preferably, ahermeticity layer is further selected to promote compatibility with anunderlying reactive metal (e.g., aluminum or aluminum alloy) electrodestructure of an acoustic resonator structure. Although aluminum oraluminum alloys are frequently used as electrode materials in BAWresonator structures, various transition and post-transition metals canbe used for such electrodes.

Following deposition of an interface layer (optionally arranged over anunderlying hermeticity layer), a SAM is preferably formed over theinterface layer. SAMs are typically formed by exposure of a solidsurface to amphiphilic molecules with chemical groups that exhibitstrong affinities for the solid surface. When an interface layercomprising a hydroxylated oxide surface is used, then organosilane SAMsare particularly preferred for attachment to the hydroxylated oxidesurface. Organosilane SAMs promote surface bonding throughsilicon-oxygen (Si—O) bonds. More specifically, organosilane moleculesinclude a hydrolytically sensitive group and an organic group and aretherefore useful for coupling inorganic materials to organic polymers.An organosilane SAM may be formed by exposing a hydroxylated oxidesurface to an organosilane material in the presence of trace amounts ofwater to form intermediate silanol groups. These groups then react withfree hydroxyl groups on the hydroxylated oxide surface to covalentlyimmobilize the organosilane. Examples of possible organosilane-basedSAMs that are compatible with interface layers incorporatinghydroxylated oxide surfaces include 3-glycidoxypropyltrimethoxysilane(GPTMS), 3-mercaptopropyltrimethoxysilane (MPTMS),3-aminopropyltrimethoxysilane (APTMS), and octadecyltrimethoxysilane(OTMS), including their ethoxy- and chloro-variants. Additional silanesthat may be used for SAMs include poly(ethylene glycol) (PEG) conjugatedvariants. Those skilled in the art will recognize that otheralternatives exist, and these alternatives are considered to be withinthe scope of the present disclosure. An exemplary SAM may include athickness in a range of at least 0.5 nm or more. Preferably, a SAMreadily binds to the locally patterned interface layer but does notreadily bind to other adjacent material layers (e.g., a hermeticitylayer, a piezoelectric material, and/or a blocking material layer).

When an electrode and/or interface layer comprising gold or anothernoble metal is used, then thiol-based (e.g., alkanethiol-based) SAMs maybe used. Alkanethiols are molecules with an S—H head group, a tailgroup, and a back bone comprising an alkyl chain. Thiols may be used onnoble metal interface layers due to the strong affinity of sulfur forthese metals. Examples of thiol-based SAMs that may be used include, butare not limited to, 1-dodecanethiol (DDT), 11-mercaptoundecanoic acid(MUA), and hydroxyl-terminated (hexaethylene glycol) undecanethiol(1-UDT). These thiols contain the same backbone, but different endgroups—namely, methyl (CH₃), carboxyl (COOH), and hydroxyl-terminatedhexaethylene glycol (HO—(CH₂CH₂O)₆) for DDT, MUA, and 1-UDT,respectively. In certain embodiments, SAMs may be formed by incubatinggold surfaces in thiol solutions using a suitable solvent, such asanhydrous ethanol.

Following formation of a SAM, the SAM may be biologicallyfunctionalized, such as by receiving at least one functionalization(e.g., specific binding) material. In certain embodiments, specificbinding materials may be applied on or over a SAM using a microarrayspotting needle or other suitable methods. In certain embodiments, aninterface layer may be patterned (e.g., using photolithographic maskingand selective etching for defining the interface layer) with a highdimensional tolerance over only a portion of a BAW resonator structure(which includes a substrate), a SAM may be applied over the interfacelayer, and a subsequently applied specific binding material may beattached only to the SAM. In certain embodiments, patterning of aninterface layer may provide a higher dimensional tolerance forpositioning of the specific binding material than could be attained bymicroarray spotting alone. Examples of specific binding materialsinclude, but are not limited to, antibodies, receptors, ligands, and thelike. A specific binding material is preferably configured to receive apredefined target species (e.g., molecule, protein, DNA, virus,bacteria, etc.). A functionalization material including specific bindingmaterial may include a thickness in a range of from about 5 nm to about1000 nm, or from about 5 nm to about 500 nm. In certain embodiments, anarray of different specific binding materials may be provided overdifferent active regions of a multi-resonator structure (i.e., one ormore resonator structures including multiple active regions), optionallyin combination with one or more active regions that are devoid ofspecific binding materials to serve as comparison (or “reference”)regions. In certain embodiments, a functionalization (e.g.,bio-functionalization) material may provide non-specific bindingutility.

Certain embodiments are directed to a fluidic device including multiplebulk acoustic wave (BAW) MEMS resonator structures as disclosed hereinand including a fluidic passage (e.g., a channel, a chamber, or thelike) arranged to conduct a liquid to contact at least onefunctionalization (e.g., specific binding) material arranged over atleast one active region of the BAW MEMS resonator structures. Such adevice may be microfluidic in scale, and may comprise at least onemicrofluidic passage (e.g., having at least one dimension, such asheight and/or width, of no greater than about 500 microns, or about 250microns, or about 100 microns). For example, following fabrication ofbulk acoustic wave MEMS resonator structures and deposition of a SAMover portions thereof (optionally preceded by deposition of ahermeticity layer and an interface layer), a microfluidic device may befabricated by forming one or more walls defining lateral boundaries of amicrofluidic passage over a first bulk acoustic wave MEMS resonatorstructure with an active region thereof arranged along a bottom surfaceof the microfluidic passage, and then enclosing the microfluidic passageusing a cover or cap layer that may define fluidic ports (e.g.,openings) enabling fluid communication with the microfluidic passage. Incertain embodiments, functionalization (e.g., specific binding) materialmay be pre-applied to the active region of a bulk acoustic wave MEMSresonator structure before formation of the microfluidic passage; inother embodiments, functionalization material may be applied over anactive region of a bulk acoustic wave resonator structure followingformation of the microfluidic passage.

In certain embodiments, a chemical or biological blocking material maybe applied over a portion of a SAM to prevent attachment of afunctionalization (e.g., specific binding) material over one or moreselected regions of a BAW resonator structure (e.g., one or more regionsapart from an active region). The proper choice of a chemical orbiological blocking material (e.g., blocking buffer) for a givenanalysis depends on the type of target species or analyte present in asample. Various types of blocking buffers such as highly purifiedproteins, serum, or milk may be used to block free sites on a SAM.Additional blockers include ethanolamine or polyethylene oxide(PEO)-containing materials. An ideal blocking buffer would bind to allpotential sites of non-specific interaction away from an active region.To optimize a blocking buffer for a particular analysis, empiricaltesting may be used to determine signal-to-noise ratio. No singlechemical or biological blocking material is ideal for every situation,since each antibody-antigen pair has unique characteristics.

FIG. 3 is a side cross-sectional schematic view of a portion of afluidic device 58 (e.g., a biochemical sensor device) fabricated withlaser-cut laminate layers including a fluidic passage 52 bounded frombelow by a base structure including a BAW resonator structure, boundedlaterally by a wall structure embodied in a pre-cut (e.g., laser-cut)wall layer 44A, and bounded from above by a cover or cap layer 46,wherein the fluidic device 58 serves as a first comparison device toprovide context for subsequently described embodiments of thedisclosure.

The fluidic device 58 includes a substrate 12 overlaid with an acousticreflector 14, and a bottom side electrode 20 arranged generally below apiezoelectric material 22. A top side electrode 28 extends over aportion of the piezoelectric material 22, wherein a portion of thepiezoelectric material 22 arranged between the top side electrode 28 andthe bottom side electrode 20 embodies an active region 30 of the BAWresonator structure. The bottom side electrode 20 is arranged along aportion of a lower surface 24 of the piezoelectric material 22. The topside electrode 28 and the piezoelectric material 22 are overlaid with ahermeticity layer 32, an interface layer 34, and a self-assembledmonolayer (SAM) 36. Portions of the SAM 36 between the active region 30and the wall layer 44A are overlaid with a chemical or biologicalblocking material 54 to prevent localized attachment offunctionalization material and/or analyte. A portion of the SAM 36 thatis registered with the active region 30 is overlaid with a layer offunctionalization (e.g., specific binding) material 38 arranged to bindat least one analyte 42. Walls of the wall layer 44A are laterallydisplaced from the active region 30 and extend upward from the blockingmaterial 54 to define lateral boundaries of the fluidic passage 52containing the active region 30. The cover or cap layer 46 definesfluidic inlet and outlet ports 48, 50 (suitable for admitting a fluidvolume 40 such as an analyte-containing sample) and is further providedto provide an upper boundary for the fluidic passage 52. The cover orcap layer 46 may be formed by defining fluidic inlet and outlet ports48, 50 (e.g., via laser cutting or water jet cutting) in a layer of anappropriate material (e.g., a substantially inert polymer, glass,silicon, ceramic, or the like), and adhering the cover or cap layer 46to top surfaces of the wall layer 44A.

The wall layer 44A is formed of a laser-cut “stencil” layer of thinpolymeric material and/or laminate material, coated with adhesivematerial 56 to promote adhesion to the underlying blocking material 54and to the overlying cover or cap layer 46. For example, the wall layer44A and the adhesive material 56 may include adhesive tape. Onechallenge associated with devices fabricated with laser cut laminates isthat excess adhesive material 56 present on one or more surfaces of thewall layer 44A is prone to “squish”—i.e., to be compressively ejectedfrom between layers. Such effect is shown in FIG. 3, in which ejectedportions 56′ of adhesive material 56 extend into the fluidic passage 52,and undesirably cover a portion of the functionalization material 38proximate to the active region 30. In extreme cases, ejected portions56′ of adhesive material 56 may interfere with operation of the fluidicdevice 58. Another challenge with laser cut laminates is difficulty inaligning the wall layer 44A and cover or cap layer 46 to one another andto the underlying base structure. The imprecise alignment results bothfrom poor tolerance of the laser-cut layers and the manual alignmentprocess, and tends to lead to architectures with larger than desiredfeature sizes.

During intended use of the fluidic device 58, a fluid volume 40 may besupplied through the fluidic inlet port 48 into the fluidic passage 52over the active region 30 and then flow through the fluidic outlet port50 to exit the fluidic passage 52. Due to the laminar nature of thefluid flow within the fluidic passage 52, the fluid volume 40 may bemodeled and behave as a “stack” of horizontal fluid layers. An analyte42 contained in one or more lower layers of the fluid volume 40 may bindwith functionalization material 38 arranged over the active region 30.Assuming that sufficient analyte is present to bind withfunctionalization material 38 arranged over the active region 30, when abulk acoustic wave having a dominant shear component is induced in theactive region 30 by supplying an electrical (e.g., alternating current)signal of a desired frequency to the bottom and top side electrodes 20,28, a change in electroacoustic response (e.g., at least one of anamplitude-magnitude property, a frequency property, or a phase property,such as a shift in resonant frequency) of the BAW resonator structuremay be detected to indicate a presence and/or quantity of analyte 42bound to the functionalization material 38.

The above-described challenges associated with fluidic devicesincorporating BAW resonator structures (e.g., biochemical sensordevices) fabricated with stencil-based wall structures have led theApplicant to utilize photosensitive materials for forming wall layerstructures. An example of a suitable photosensitive material is an epoxymaterial such SU-8, which can form precisely dimensioned structures withhigh height/width aspect ratios, and has excellent biomedicalcompatibility. In use, a photosensitive material may be applied over asurface, a photomask may be placed thereover, and energy such asultraviolet emissions or proton beams may be transmitted throughopenings in the photomask to selectively cure the photosensitivematerial to form microstructures. Beyond SU-8, other suitable materialsfor forming photo-defined wall layer structures include TMMF epoxy(e.g., a high resolution permanent dry film photoresist composed of 5%antimony compound and 95% novolak-type epoxy resin) as well as otherphotoresist and solder mask materials.

FIG. 4A is a schematic cross-sectional view of a portion of a fluidicdevice 60 (e.g., a biochemical sensor device) including a fluidicpassage 52 bounded from below by a base structure including a BAWresonator structure, bounded laterally by a wall structure 44 fabricatedof photosensitive (e.g., epoxy or photoresist) materials, and boundedfrom above by a cover or cap layer 46. For example, the wall structure44 may be fabricated of SU-8 epoxy. The fluidic device 60 serves as asecond comparison device intended to provide context for subsequentlydescribed embodiments of the disclosure. As compared to the fluidicdevice 58 of FIG. 3, the fluidic device 60 of FIG. 4A lacks adhesivematerial 56 between the wall structure 44 and the adjacent structures,such that the fluidic device 60 does not exhibit any compressiveejection or “squish” of adhesive between layers.

With continued reference to FIG. 4A, the fluidic device 60 includes asubstrate 12 overlaid with an acoustic reflector 14, and a bottom sideelectrode 20 arranged generally below a piezoelectric material 22. A topside electrode 28 extends over a portion of the piezoelectric material22, wherein a portion of the piezoelectric material 22 arranged betweenthe top side electrode 28 and the bottom side electrode 20 embodies anactive region 30 of the BAW resonator structure. The bottom sideelectrode 20 is arranged along a portion of a lower surface 24 of thepiezoelectric material 22. The top side electrode 28 and thepiezoelectric material 22 are overlaid with a hermeticity layer 32, aninterface layer 34, and a self-assembled monolayer (SAM) 36. Portions ofthe SAM 36 between the active region 30 and the wall structure 44 areoverlaid with a chemical or biological blocking material 54 to preventlocalized attachment of functionalization material and/or analyte. Aportion of the SAM 36 that is registered with the active region 30 isoverlaid with a layer of functionalization (e.g., specific binding)material 38 arranged to bind at least one analyte 42. Walls of the wallstructure 44 are laterally displaced from the active region 30 andextend upward from the SAM 36 to define lateral boundaries of thefluidic passage 52 containing the active region 30. The cover or caplayer 46 defines fluidic inlet and outlet ports 48, 50 (suitable foradmitting a fluid volume 40 such as an analyte-containing sample) and isfurther provided to provide an upper boundary for the fluidic passage52. The cover or cap layer 46 may be fabricated of a photosensitivematerial, or may be fabricated of other materials such as machined glassor silicon, or composite material. Operation of the fluidic device 60 issubstantially similar to the operation of the fluidic device 58described in connection with FIG. 3.

While photosensitive materials such as SU-8 can provide structures withprecisely defined features, stress and adhesion embody challenges whenfabricating wall structures from such materials. For example, SU-8 has ahigh degree of stress relative to an underlying substrate. Intrinsicstress is generated during crosslinking, and extrinsic stress is imposeddue to a coefficient of thermal expansion (CTE) mismatch between SU-8and the underlying substrate. These stresses and the thickness of a wallstructure fabricated with SU-8 apply a moment (force times distance(exerted over the height of a wall structure), resulting in applicationof torque) on a joint between the wall structure and the underlying basestructure (e.g., including a substrate or layers deposited over asubstrate). This moment can tend to delaminate a wall structure from anunderlying base structure, thereby opening the joint therebetween, andtending to compromise structural and/or sealing integrity of a fluidicdevice incorporating a BAW resonator structure.

Delamination between the wall structure 44 and the SAM 36 of a basestructure incorporating the BAW resonator structure of the fluidicdevice 60 is shown in FIG. 4B. FIG. 4B is a schematic cross-sectionalview of the fluidic device portion of FIG. 4A, showing a delaminationcrack 62 between a left side wall structure 44 and the SAM 36 uponapplication of a moment caused by intrinsic and extrinsic stress of thewall structure 44, with the moment equaling the product of the force Fand the distance d. Additionally, SU-8 can absorb liquid, and liquidabsorption can change the stress levels. Thus, delamination (e.g.,opening or “unzipping” of a bond joint) may be hastened when the wallstructure 44 is exposed to fluids and/or humid operating environments.

FIG. 5 is a scanning electron microscope (10,000 times magnification) ofa base portion of a photosensitive material (e.g., epoxy- orresist-based) wall structure 44 proximate to a base structure (e.g.,including a SAM 36 along an upper surface thereof), showing adelamination crack 62 between the wall structure 44 and the basestructure after exposure to a humidity source.

In certain embodiments, a wall structure (e.g., fabricated ofphotosensitive material such as SU-8 epoxy) may include a footer portionand an upper wall portion extending upward therefrom, with the footerportion having a width that exceeds a width of the upper wall portion. Alateral edge of the footer portion is preferably non-coincident with,and outwardly displaced relative to, a lateral edge of the upper wallportion. Additionally, a footer portion is preferably thinner than anupper wall portion of a wall structure. In one exemplary embodiment, afooter portion may include a thickness in a range of from 1 to 20microns, and an upper wall portion may include a thickness in a range offrom 10 to 100 microns. In certain embodiments, an upper wall portionmay be from 5 to 15 times thicker than a footer portion of a wallstructure. Providing a wider footer portion underlying the upper wallportion tends to reduce the risk of delamination or peeling at aninterface between the wall structure and an underlying base structure,since any moment applied by the upper wall portion is preferably nottransmitted a lateral edge of the footer portion. Additionally, aninterface between a footer portion and an upper wall portion maycharacterized by a high degree of adhesion, particularly if suchportions comprise the same material. Moreover, fabricating the wallstructure in multiple parts may reduce intrinsic stress generated duringmanufacture. The footer portion may also serve as a stress relief layer.The net result is to increase robustness of adhesion between a wallstructure and an underlying base structure, therefore reducing the riskof delamination and peeling between such structures.

FIG. 6A is a schematic cross-sectional view of a portion of a fluidicdevice 66 (e.g., a biochemical sensor device) including a fluidicpassage 52 bounded from below by a base structure including a BAWresonator structure, bounded from above by a cover or cap layer 46, andbounded laterally by a wall structure fabricated of photosensitive(e.g., photo-defined epoxy or resist) materials including a wider footerportion 64 and a narrower upper wall portion 44′ both fabricated withphoto-defined epoxy or resist materials, according to one embodiment.The fluidic device 66 includes a substrate 12 overlaid with an acousticreflector 14, and a bottom side electrode 20 arranged generally below apiezoelectric material 22. A top side electrode 28 extends over aportion of the piezoelectric material 22, wherein a portion of thepiezoelectric material 22 arranged between the top side electrode 28 andthe bottom side electrode 20 embodies an active region 30 of the BAWresonator structure. The bottom side electrode 20 is arranged along aportion of a lower surface 24 of the piezoelectric material 22. The topside electrode 28 and the piezoelectric material 22 are overlaid with ahermeticity layer 32, an interface layer 34, and a self-assembledmonolayer (SAM) 36. Portions of the SAM 36 between the active region 30and the footer portion 64 are overlaid with a chemical or biologicalblocking material 54 to prevent localized attachment offunctionalization material and/or analyte. A portion of the SAM 36 thatis registered with the active region 30 is overlaid with a layer offunctionalization (e.g., specific binding) material 38 arranged to bindat least one analyte 42. Wall structures consisting of a wider footerportion 64 and a narrower upper wall portion 44′ are laterally displacedfrom the active region 30 and extend upward from the SAM 36 to definelateral boundaries of the fluidic passage 52 containing the activeregion 30. The cover or cap layer 46 defines fluidic inlet and outletports 48, 50 (suitable for admitting a fluid volume 40 such as ananalyte-containing sample) and is further provided to provide an upperboundary for the fluidic passage 52. FIG. 6B is a magnifiedcross-sectional schematic view of an upper portion of the fluidic device66 shown in FIG. 6A. Operation of the fluidic device 66 is similar tothe operation of the fluidic device 58 described in connection with FIG.3.

In certain embodiments, peel resistance is enhanced by providing a wallstructure (e.g., fabricated of photosensitive material such as SU-8epoxy) arranged over at least one anchoring region of a base structure,wherein the at least one anchoring region includes at least oneanchoring feature, and the at least one anchoring feature includes atleast one recess and/or at least one protrusion (optionally, multiplerecesses and/or multiple protrusions). Presence of one or more anchoringregions promotes stronger adhesion between a wall structure and anunderlying base structure (whether or not used in combination with awall structure embodied in a footer portion and an upper wall portion asdescribed above). In certain embodiments, multiple protrusions and/orrecesses of an anchoring region may be embodied in a textured surfacehaving a repeating textural pattern. In certain embodiments, eachanchoring feature comprises a vertical dimension of least about 1micron. Protrusions and/or recesses of an anchoring region may be formedin or on a base structure by methods such as selective etching (e.g.,preceded by photolithographic patterning), three-dimensional printing,laser micromachining, selective deposition, and the like. Moregenerally, protrusions and/or recesses of an anchoring region may beformed by a subtractive material removal process (e.g., etching, lasermicromachining, etc.), and/or an additive manufacturing process (e.g.,involving deposition of materials such as SU-8, photoresist, Parylene,epoxy, polymers, etc.). In certain embodiments, protrusions and/orrecesses of an anchoring region may be defined prior to application ofone or more of: a hermeticity layer, an interface layer, aself-assembled monolayer, a blocking material, or any other desiredlayer.

FIG. 7 is a schematic cross-sectional view of a portion of a fluidicdevice 76 (e.g., a biochemical sensor device) including a fluidicpassage 52 bounded from below by a base structure including a BAWresonator structure, bounded from above by a cover or cap layer 46, andbounded laterally by a wall structure 44 fabricated with photo-definedepoxy or resist materials, with the wall structure 44 overlyinganchoring regions 68 each including recesses 74 and/or protrusions 70defined in or on the base structure, according to one embodiment. Incertain embodiments, each protrusion 70 includes an upwardly extendingsegment 72 of an underlying layer (e.g., an interface layer 34) that isoverlaid with a substantially continuous self-assembled monolayer 36.

The fluidic device 76 includes a substrate 12 overlaid with an acousticreflector 14, and a bottom side electrode 20 arranged generally below apiezoelectric material 22. A top side electrode 28 extends over aportion of the piezoelectric material 22, wherein a portion of thepiezoelectric material 22 arranged between the top side electrode 28 andthe bottom side electrode 20 embodies an active region 30 of the BAWresonator structure. The bottom side electrode 20 is arranged along aportion of a lower surface 24 of the piezoelectric material 22. The topside electrode 28 and the piezoelectric material 22 are overlaid with ahermeticity layer 32, an interface layer 34, and a self-assembledmonolayer (SAM) 36. Portions of the SAM 36 between the active region 30and the wall structure 44 are overlaid with a chemical or biologicalblocking material 54 to prevent localized attachment offunctionalization material and/or analyte. A portion of the SAM 36 thatis registered with the active region 30 is overlaid with a layer offunctionalization (e.g., specific binding) material 38 arranged to bindat least one analyte 42. Anchoring regions 68 include protrusions 70 andrecesses 74, and are laterally displaced from (thereby beingnon-coincident with) the active region 30. The wall structure 44 extendsupward from the anchoring regions 68 to define lateral boundaries of thefluidic passage 52 containing the active region 30. The cover or caplayer 46 defines fluidic inlet and outlet ports 48, 50 (suitable foradmitting a fluid volume 40 such as an analyte-containing sample) and isfurther provided to provide an upper boundary for the fluidic passage52. Operation of the fluidic device 76 is substantially similar to theoperation of the fluidic device 58 described in connection with FIG. 3.

FIG. 8A is a magnified schematic cross-sectional view of a singleprotrusion 70A (i.e., an anchoring feature) formed by an interface layer34 and an overlying self-assembled monolayer (SAM) 36 of a fluidicdevice, according to one embodiment. The protrusion 70A includes anupwardly extending portion 72′ of the interface layer 34, with theupwardly extending portion 72′ being overlaid with the SAM 36. Incertain embodiments, the interface layer 34 may be initially depositedwith increased thickness, and regions of such material may beselectively removed (via any suitable subtractive material removalprocess) to form upwardly extending protrusions separated by troughs,whereby subtractive removal removes less than an entire thickness of theinterface layer 34. In other embodiments, subtractive removal locallyremoves the entire thickness of the interface layer 34.

FIG. 8B is a magnified schematic cross-sectional view of a singleprotrusion 70B (i.e., an anchoring feature) formed by a depositedmaterial 78 (e.g., photosensitive or photoimageable material) extendingupward from a surface of an interface layer 34 and being overlaid with aself-assembled monolayer (SAM) 36, according to one embodiment. Examplesof materials that might be used for the deposited material 78 include,but are not limited to SU-8, photoresist, Parylene, epoxy, and polymers.In certain embodiments, a deposited material 78 may be applied overspecified areas using an additive manufacturing process, and thereafterportions of the deposited material 78 may be removed using a subtractiveprocess. In certain embodiments, the deposited material 78 comprises aphotoimageable material to facilitate patterning.

FIGS. 9A-9E provide schematic cross-sectional views of a portion of aninterface layer 82 with recesses in various states of formation in anupper surface thereof using a process such as photolithographicpatterning followed by selective etching to form anchoring features.FIG. 9A illustrates the interface layer 82 overlaid with a layer ofphotoresist 84, with a photomask 86 defining mask windows 88 arrangedbetween the layer of photoresist 84 and an electromagnetic (e.g.,ultraviolet) radiation source 90. FIG. 9B illustrates the photomask 86,interface layer 82, and layer of photororesist 84 following impingementof radiation through the mask windows 88 to form soluble regions 92 inthe layer of photoresist 84. Such soluble regions 92 may be removed byapplication of a suitable developer chemical to yield a layer ofphotoresist 84 defining photoresist windows 92′, as shown in FIG. 9C.Thereafter, a suitable etchant may be applied through the photoresistwindows 92′ to form grooves or recesses 96 in the interface layer 82, asshown in FIG. 9D. Finally, the layer of photoresist 84 may be removed toyield an interface layer 82 including an exposed upper surface 94′ andgrooves or recesses 96 that extend from the upper surface 94′ into aninterior of the interface layer 82, as shown in FIG. 9E. The resultinggrooves or recesses 96 are separated by elevated regions or protrusions94, with the foregoing elements being useable as anchoring features topromote adhesion of an overlying wall structure (not shown) bounding afluidic passage of a fluidic device (e.g., a biosensor device). AlthoughFIG. 9E shows the grooves or recesses 96 as extending through only aportion of a thickness of the interface layer 82, in certainembodiments, one or more grooves or recesses 96 may extend through theentire thickness of the interface layer 82.

FIG. 10 is a schematic cross-sectional view of a portion of a fluidicdevice 98 (e.g., a biochemical sensor device) including a fluidicpassage 52 bounded from below by a base structure including a BAWresonator structure, bounded from above by a cover of cap layer 46, andbounded laterally by a wall structure fabricated with photo-definedepoxy or resist materials, with the wall structure including a footerportion 64 having a width that exceeds a width of an upper wall portion44′, and with the footer portion 64 overlying anchoring regions 68including recesses 74 and/or protrusions 70 defined in or on the basestructure, according to one embodiment. Use of a wall structureincluding a footer portion 64 (e.g., according to FIGS. 6A and 6B) andincluding anchoring regions 68 (e.g., according to FIG. 7) may providefurther enhanced peeling resistance relative to use of one of thesefeatures alone.

The fluidic device 98 includes a substrate 12 overlaid with an acousticreflector 14, and a bottom side electrode 20 arranged generally below apiezoelectric material 22. A top side electrode 28 extends over aportion of the piezoelectric material 22, wherein a portion of thepiezoelectric material 22 arranged between the top side electrode 28 andthe bottom side electrode 20 embodies an active region 30 of the BAWresonator structure. The bottom side electrode 20 is arranged along aportion of a lower surface 24 of the piezoelectric material 22. The topside electrode 28 and the piezoelectric material 22 are overlaid with ahermeticity layer 32, an interface layer 34, and a self-assembledmonolayer (SAM) 36. Portions of the SAM 36 between the active region 30and the upper wall portion 44′ are overlaid with a chemical orbiological blocking material 54 to prevent localized attachment offunctionalization material and/or analyte. A portion of the SAM 36 thatis registered with the active region 30 is overlaid with a layer offunctionalization (e.g., specific binding) material 38 arranged to bindat least one analyte 42. Anchoring regions 68 include protrusions 70 andrecesses 74, and are laterally displaced from (thereby beingnon-coincident with) the active region 30. Each protrusion 70 includesan upwardly extending segment 72 of an underlying layer (e.g., aninterface layer 34) that is overlaid with the substantially continuousSAM 36. The footer portion 64 of the wall structure extends upward fromthe anchoring regions 68, and the upper wall portion 44′ extends upwardfrom the footer portion 64, to define lateral boundaries of the fluidicpassage 52 containing the active region 30. The cover or cap layer 46defines fluidic inlet and outlet ports 48, 50 (suitable for admitting afluid volume 40 such as an analyte-containing sample) and is furtherprovided to provide an upper boundary for the fluidic passage 52.Operation of the fluidic device 98 is substantially similar to theoperation of the fluidic device 58 described in connection with FIG. 3.FIG. 11A is a schematic cross-sectional view of a film bulk acousticwave resonator (FBAR) structure 100 including an active region 30,wherein at least portions of the active region 30 are subject to beingoverlaid with an interface layer and a self-assembled monolayer (SAM)suitable for receiving a functionalization (e.g., specific binding ornon-specific binding) material, according to one embodiment. The FBARstructure 100 includes a substrate 102 (e.g., silicon or anothersemiconductor material) defining a cavity 104 optionally covered by asupport layer 106 (e.g., silicon dioxide). A bottom side electrode 20 isarranged over a portion of the support layer 106, a piezoelectricmaterial 22, preferably embodying inclined c-axis hexagonal crystalstructure piezoelectric material (e.g., AlN or ZnO), is arranged overthe bottom side electrode 20 and the support layer 106, and a top sideelectrode 28 is arranged over at least a portion of a top surface of thepiezoelectric material 22. A portion of the piezoelectric material 22arranged between the top side electrode 28 and the bottom side electrode20 embodies the active region 30 of the FBAR structure 100. The activeregion 30 is arranged over and registered with the cavity 104 disposedbelow the support layer 106. The cavity 104 serves to confine acousticwaves induced in the active region 30 by preventing dissipation ofacoustic energy into the substrate 102, since acoustic waves do notefficiently propagate across the cavity 104. In this respect, the cavity104 provides an alternative to the acoustic reflector 14 illustrated inFIGS. 1, 3-4B, 6A, 7, and 10. Although the cavity 104 shown in FIG. 11Ais bounded from below by a thinned portion of the substrate 102, inalternative embodiments at least a portion of the cavity 104 may extendthrough an entire thickness of the substrate 102. Steps for forming theFBAR structure 100 may include defining the cavity 104 in the substrate102, filling the cavity 104 with a sacrificial material (not shown)optionally followed by planarization of the sacrificial material,depositing the support layer 106 over the substrate 102 and thesacrificial material, removing the sacrificial material (e.g., byflowing an etchant through vertical openings defined in the substrate102 or the support layer 106, or lateral edges of the substrate 102),depositing the bottom side electrode 20 over the support layer 106,growing (e.g., via sputtering or other appropriate methods) thepiezoelectric material 22, and depositing the top side electrode 28. Incertain embodiments, the top side electrode 28, the piezoelectricmaterial 22, and the bottom side electrode 20 in combination may beself-supporting, and the support layer 106 may be omitted and/or removedby etching in the vicinity of the active region 30.

FIG. 11B is a schematic cross-sectional view of the FBAR structure 100according to FIG. 11A, following addition of a hermeticity layer 32, aninterface layer 34, a self-assembled monolayer (SAM) 36, andfunctionalization material 38 (e.g., specific binding material). Thehermeticity layer 32 is arranged over the entire piezoelectric material22 (as well as the top side electrode 28), whereas the functionalizationmaterial 38, the SAM 36, and the interface layer 34 are arranged solelyover the active region 30. As shown in FIG. 11B, analyte 42 is bound tothe functionalization material 38, such as may occur following exposureof the functionalization material 38 to a medium (e.g., liquid or otherfluid) containing the analyte 42, optionally as part of a microfluidicdevice.

As will be recognized by one skilled in the art upon review of thepresent disclosure, in certain embodiments, the FBAR structure 100 ofFIGS. 11A and 11B may be substituted for the solidly mounted BAWresonator structures disclosed previously herein. In certainembodiments, the FBAR structure 100 of FIG. 11B may be incorporated in afluidic device including composite wall structures (e.g., including afooter portion and an upper wall portion) and/or anchoring regions asdisclosed herein, in order to promote persistent bonding between a wallstructure and a base structure.

FIG. 12 is a top plan view photograph of a bulk acoustic wave MEMSresonator device 10 (consistent with the portion of the resonator device10 illustrated in FIG. 1) suitable for receiving a hermeticity layer, aninterface layer, a self-assembled monolayer, and/or functionalization(e.g., specific binding) material as disclosed herein, wherein the MEMSresonator device 10 may serve as a base structure of a fluidic device asdisclosed herein. The MEMS resonator device 10 includes a piezoelectricmaterial (not shown) arranged over a substrate 12, a bottom sideelectrode 20 arranged under a portion of the piezoelectric material, anda top side electrode 28 arranged over a portion of the piezoelectricmaterial, including an active region 30 in which the piezoelectricmaterial is arranged between overlapping portions of the top sideelectrode 28 and the bottom side electrode 20. Externally accessiblecontacts 20A, 28A are in electrical communication with the bottom sideelectrode 20 and the top side electrode 28, respectively. After portionsof the resonator device 10 are overlaid with an interface layer, aself-assembled monolayer, and functionalization (e.g., specific binding)material as disclosed herein, the resonator device 10 may be used as asensor and/or incorporated into a microfluidic device, with wallstructures fabricated of photosensitive materials such as SU-8. Ifdesired, multiple resonator devices 10 may be provided in an array on asingle substrate 12.

FIG. 13 is a perspective assembly view of a base structure 110 includingmultiple bulk acoustic wave MEMS resonator structures as disclosedherein, suitable for receiving a wall structure and a cover structure asdisclosed herein in order to fabricate a multi-resonator fluidic device.The base structure 110 includes a substrate 112. Top central portions ofthe substrate 112, which includes an acoustic reflector (not shown) anda piezoelectric material (not shown), include a top side electrode 116and bottom side electrodes 114A-114N. Regions in which the foregoingelectrodes overlap one another and sandwich the piezoelectric materialembody active regions 118A-118N. Any suitable number of active regions118A-118N may be provided and fluidically arranged in series orparallel, although four active regions are illustrated in FIG. 13. Topperipheral (or top end) portions of the substrate 112 further includereference top side electrodes 126 and reference bottom side electrodes124 in communication with reference overlap regions 120. Such referenceoverlap regions 120 are not intended to be exposed to fluid, and arepresent to provide a basis for comparing signals obtained from theactive regions 118A-118N exposed to fluid when one or more fluidicchannels are defined over the base structure 110.

Technical benefits obtainable with various embodiments of the presentdisclosure may include enhanced resistance of peeling and delaminationof precisely dimensioned wall structures of fluidic devicesincorporating bulk acoustic wave resonators, including devices suitablefor biosensing or biochemical sensing applications.

Those skilled in the art will recognize improvements and modificationsto the preferred embodiments of the present disclosure. All suchimprovements and modifications are considered within the scope of theconcepts disclosed herein and the claims that follow.

1.-10. (canceled)
 11. A fluidic device comprising: a base structurecomprising: (i) a substrate; and (ii) at least one bulk acoustic waveresonator structure supported by the substrate, the at least one bulkacoustic wave resonator structure including a piezoelectric material, atop side electrode arranged over a portion of the piezoelectricmaterial, and a bottom side electrode arranged below at least a portionof the piezoelectric material, wherein a portion of the piezoelectricmaterial is arranged between the top side electrode and the bottom sideelectrode to form an active region, and wherein a portion of the basestructure comprises at least one anchoring region including at least oneanchoring feature, and the at least one anchoring feature comprises atleast one of: (i) at least one recess or (ii) at least one protrusion;and a wall structure arranged over the at least one anchoring region anddefining lateral boundaries of a fluidic passage arranged to receive afluid and containing the active region.
 12. The fluidic device of claim11, wherein the at least one anchoring feature comprises a verticaldimension of least about 1 micron.
 13. The fluidic device of claim 11,wherein the at least one recess comprises a plurality of recesses, andthe at least one protrusion comprises a plurality of protrusions. 14.The fluidic device of claim 11, further comprising a cover structurearranged over the wall structure and defining an upper boundary of thefluidic passage.
 15. The fluidic device of claim 14, wherein the wallstructure and the cover structure are embodied in a monolithic bodystructure.
 16. The fluidic device of claim 11, wherein the wallstructure comprises at least one of a photosensitive material,photoresist, or epoxy.
 17. The fluidic device of claim 11, furthercomprising at least one functionalization material arranged over atleast a portion of the active region.
 18. The fluidic device of claim17, further comprising a self-assembled monolayer arranged between theat least one functionalization material and the top side electrode. 19.The fluidic device of claim 18, further comprising an interface layerarranged between the self-assembled monolayer and the top sideelectrode.
 20. The fluidic device of claim 19, further comprising ahermeticity layer arranged between the interface layer and the top sideelectrode.
 21. A method for biological or chemical sensing, the methodcomprising: supplying a fluid containing an analyte into the fluidicpassage of the fluidic device according to claim 16, wherein saidsupplying is configured to cause at least some of the analyte to bind tothe at least one functionalization material; inducing a bulk acousticwave in the active region; and sensing a change in at least one of anamplitude-magnitude property, a frequency property, or a phase propertyof the at least one bulk acoustic wave resonator structure to indicateat least one of presence or quantity of target species bound to the atleast one functionalization material.